Preparation method of trichloromethanesulfonic acid

Abstract

The invention discloses a preparation method of trichloromethanesulfonic acid. The method comprises the following steps: taking methanesulfonic acid and chlorine as raw materials, adding the methanesulfonic acid and chlorine into a reactor according to a molar ratio of 1: (3-10), illuminating and heating the methanesulfonic acid and chlorine as raw materials in the reactor at 150-500 DEG C, and chloridizing the methanesulfonic acid through chlorine in the tubular reactor to obtain trichloromethanesulfonic acid. The method for preparing the trichloromethanesulfonic acid is simple in process, convenient to operate, high in yield and stable in product quality, the purity of the prepared trichloromethanesulfonic acid is higher than 98%, and the requirement of industrial production for the product quality is met.

Description

Technical Field

[0001] This invention relates to the field of organic synthesis technology, and in particular to a method for preparing trichloromethanesulfonic acid. Background Technology

[0002] Trichloromethanesulfonic acid is an important organic synthesis intermediate with wide applications in pharmaceuticals, pesticides, dyes and other fields.

[0003] For example, trichloromethanesulfonic acid can be directly used in subsequent fluorination processes to prepare trifluoromethanesulfonic acid.

[0004] However, traditional methods for preparing trichloromethanesulfonic acid suffer from problems such as complex processes, low yields, unstable product quality, and significant environmental pollution, which limit its industrial production. Summary of the Invention

[0005] To address the above problems, this invention provides a method for preparing trichloromethanesulfonic acid, which improves the yield of trichloromethanesulfonic acid and reduces the emission of harmful substances.

[0006] The present invention discloses a method for preparing trichloromethanesulfonic acid, wherein the raw materials are methanesulfonic acid and chlorine, and the molar ratio of methanesulfonic acid to chlorine is 1:3-10. Methanesulfonic acid and chlorine are added to a reactor, and the raw materials methanesulfonic acid and chlorine in the reactor are irradiated and heated to a temperature of 150-500°C. In the tubular reactor, methanesulfonic acid is chlorinated with chlorine to obtain trichloromethanesulfonic acid.

[0007] According to the method for preparing trichloromethanesulfonic acid, a tubular reactor is used. The raw materials methanesulfonic acid and chlorine react inside the outer tube of the tubular reactor. Light is irradiated outside the outer tube of the tubular reactor, and a temperature-controlled medium flows inside the inner tube of the tubular reactor.

[0008] According to the method for preparing trichloromethanesulfonic acid, the inner diameter of the tubular reactor is 5-20 mm, the inner diameter of the outer tube is 2-5 mm larger than that of the inner tube, and the length-to-diameter ratio of the inner tube is 500-3000.

[0009] According to the method for preparing trichloromethanesulfonic acid, the illumination uses an ultraviolet lamp with a power of 10-100W and a wavelength of 250-450nm.

[0010] According to the method for preparing trichloromethanesulfonic acid, the feed rate of methanesulfonic acid is 0.2-3 g / min.

[0011] According to the method for preparing trichloromethanesulfonic acid, the temperature control medium is a heat transfer oil, which can be silicone oil, mineral oil, or synthetic oil.

[0012] According to the method for preparing trichloromethanesulfonic acid, the high-temperature heating temperature is 150-500℃.

[0013] The beneficial effects achieved by this invention are as follows: 1. The application of tubular reactors makes the reaction process more efficient and controllable.

[0014] 2. The combination of light and high temperature conditions not only increases the reaction rate, but also helps to improve the purity and stability of the product.

[0015] 3. The trichloromethanesulfonic acid prepared by this invention has a purity higher than 98%, meeting the quality requirements for industrial production. This method also has advantages such as simple operation and stable process, opening up new avenues for the preparation of trichloromethanesulfonic acid and its derivatives. Detailed Implementation

[0016] The following examples further illustrate the above-described content of the present invention, but it should not be construed as limiting the scope of the subject matter of the present invention to the following examples. All technologies implemented based on the above-described content of the present invention fall within the scope of the present invention.

[0017] The present invention discloses a method for preparing trichloromethanesulfonic acid, wherein the raw materials are methanesulfonic acid and chlorine, and the molar ratio of methanesulfonic acid to chlorine is 1:3-10. The methanesulfonic acid and chlorine are introduced into a tubular reactor, and the raw materials methanesulfonic acid and chlorine in the tubular reactor are irradiated and heated to a temperature of 150-500°C. The methanesulfonic acid in the tubular reactor is chlorinated with chlorine to obtain trichloromethanesulfonic acid.

[0018] The tubular reactor used in this invention has an inner tube diameter of 5-20 mm, an outer tube inner diameter that is 2-5 mm larger than the inner tube inner diameter, and an inner tube length-to-diameter ratio of 500-3000. Ultraviolet lamps with a power of 10-100W and a wavelength of 250-450 nm are used for illumination.

[0019] The feed rate of methanesulfonic acid is 0.2-3 g / min.

[0020] The temperature control medium for tubular reactors is heat transfer oil, which can be silicone oil, mineral oil, or synthetic oil. Example 1

[0021] The tubular reactor (inner tube diameter 5mm, outer tube inner diameter 8mm, length 5m), power pump, and corresponding pipelines were fixed and connected according to experimental requirements. An ultraviolet lamp was also fixed. The heating device for the temperature-controlled medium was turned on, heating the silicone oil to 350℃. After the temperature-controlled medium reached the required temperature, the power pump was turned on to circulate the medium into the inner layer of the tubular reactor. The ultraviolet lamp was turned on, with a power setting of 50W and a wavelength of 395nm. Methanesulfonic acid and chlorine were fed into the outer layer of the tubular reactor at feed rates of 0.5g / min and 470ml / min, respectively, for reaction. The residence time of the raw materials in the inner tube of the tubular reactor was approximately 10 seconds. The resulting liquid was collected, and testing showed that the purity of trichloromethanesulfonic acid reached 98.12%, meeting the requirements for industrial production. Example 2

[0022] The tubular reactor (inner tube diameter 10mm, outer tube inner diameter 15mm, length 15m), power pump, and corresponding pipelines were fixed and connected according to experimental requirements. An ultraviolet lamp was also fixed. The heating device for the temperature-controlled medium was turned on, heating the mineral oil to 450℃. After the temperature-controlled medium reached the desired temperature, the power pump was turned on to circulate the medium into the inner layer of the tubular reactor. The ultraviolet lamp was turned on, with the power set to 80W and the wavelength to 300nm. Methanesulfonic acid and chlorine were fed into the outer layer of the tubular reactor at feed rates of 2g / min and 2000ml / min, respectively, for reaction. The residence time of the raw materials in the inner tube of the tubular reactor was approximately 15 seconds. The resulting liquid was collected, and testing showed that the purity of trichloromethanesulfonic acid reached 98.56%, meeting the requirements for industrial production. Example 3

[0023] The tubular reactor (inner tube diameter 12mm, outer tube inner diameter 15mm, length 15m), power pump, and corresponding pipelines were fixed and connected according to experimental requirements. An ultraviolet lamp was also fixed. The temperature-controlled medium heating device was turned on, heating the synthetic oil to 500℃. After the temperature-controlled medium reached the required temperature, the power pump was turned on to circulate the medium into the inner layer of the tubular reactor. The ultraviolet lamp was turned on, with a power setting of 90W and a wavelength of 275nm. Methanesulfonic acid and chlorine were fed into the outer layer of the tubular reactor at feed rates of 2.5g / min and 1200ml / min, respectively, for reaction. The residence time of the raw materials in the inner tube of the tubular reactor was approximately 20 seconds. The resulting liquid was collected, and testing showed that the purity of trichloromethanesulfonic acid reached 98.89%, meeting the requirements for industrial production. Example 4

[0024] The tubular reactor (inner tube diameter 10mm, outer tube inner diameter 15mm, length 8m), power pump, and corresponding pipelines were fixed and connected according to experimental requirements. An ultraviolet lamp was also fixed. The temperature-controlled medium heating device was turned on, heating the temperature-controlled medium, silicone oil, to 300℃. After the temperature-controlled medium reached the required temperature, the power pump was turned on to circulate the temperature-controlled medium into the inner layer of the tubular reactor. The ultraviolet lamp was turned on, with the power set to 60W and the wavelength to 350nm. Methanesulfonic acid and chlorine were fed into the outer layer of the tubular reactor at feed rates of 1g / min and 940ml / min, respectively, for reaction. The residence time of the raw materials in the inner tube of the tubular reactor was approximately 12 seconds. The resulting liquid was collected, and testing showed that the purity of trichloromethanesulfonic acid reached 98.35%, meeting the requirements for industrial production. Example 5

[0025] The tubular reactor (inner tube diameter 18mm, outer tube inner diameter 20mm, length 12m), power pump, and corresponding pipelines were fixed and connected according to experimental requirements. An ultraviolet lamp was also fixed. The temperature-controlled medium heating device was turned on, heating the temperature-controlled medium, mineral oil, to 200℃. After the temperature-controlled medium reached the required temperature, the power pump was turned on to circulate the temperature-controlled medium into the inner layer of the tubular reactor. The ultraviolet lamp was turned on, with the power set to 90W and the wavelength to 420nm. Methanesulfonic acid and chlorine were fed into the outer layer of the tubular reactor at feed rates of 1.2g / min and 1300ml / min, respectively, for reaction. The residence time of the raw materials in the inner tube of the tubular reactor was approximately 14 seconds. The resulting liquid was collected, and testing showed that the purity of trichloromethanesulfonic acid reached 98.65%, meeting the requirements for industrial production. Comparative Example 1

[0026] The tubular reactor (inner tube diameter 5mm, outer tube inner diameter 8mm, length 5m), power pump, and corresponding pipelines were fixed and connected according to experimental requirements. An ultraviolet lamp was also fixed. The temperature-controlled medium heating device was turned on, heating the temperature-controlled medium, silicone oil, to 350℃. After the temperature-controlled medium reached the required temperature, the power pump was turned on to circulate the temperature-controlled medium into the inner layer of the tubular reactor. Methanesulfonic acid and chlorine gas were fed into the outer layer of the tubular reactor at feed rates of 0.5g / min and 470ml / min, respectively, for reaction. The residence time of the raw materials in the inner tube of the tubular reactor was approximately 10 seconds. The resulting liquid was collected, and testing showed that the purity of trichloromethanesulfonic acid reached 50.95%. Comparative Example 2

[0027] The tubular reactor (inner tube diameter 5mm, outer tube inner diameter 8mm, length 5m), power pump, and corresponding pipelines were fixed and connected according to experimental requirements. The ultraviolet lamp was also fixed. The ultraviolet lamp was turned on, with the power set to 50W and the wavelength to 395nm. Methanesulfonic acid and chlorine gas were fed into the inner layer of the tubular reactor at feed rates of 0.5g / min and 470ml / min, respectively. The residence time of the raw materials in the inner tube of the tubular reactor was approximately 10 seconds. The resulting liquid was collected, and testing showed that the purity of trichloromethanesulfonic acid reached 38.12%. Comparative Example 3

[0028] The four-necked flask was fixed in the temperature-controlled medium, and the flask, power pump, and corresponding piping were secured according to experimental requirements. The UV lamp was also fixed. The UV lamp was turned on, with the power set to 50W and the wavelength to 395nm. Methanesulfonic acid and chlorine gas were fed into the four-necked flask at feed rates of 0.5g / min and 470ml / min, respectively, for reaction. The residence time of the raw materials in the tubular reactor was approximately 10 seconds. The reacted liquid was collected, and the purity of the trichloromethanesulfonic acid was determined to be 43.29%.

[0029]

[0030] This invention discloses a method for preparing trichloromethanesulfonic acid. This method uses a tubular reactor as the core equipment and achieves efficient and high-purity preparation of trichloromethanesulfonic acid through precise control of reaction conditions. This method not only simplifies the cumbersome steps of traditional preparation processes but also significantly improves product quality and yield, providing strong support for industrial production. It opens up new avenues for the preparation of trichloromethanesulfonic acid and its derivatives.

[0031] The preferred embodiments of the present invention have been described in detail above; however, the present invention is not limited thereto. Within the scope of the inventive concept, various simple modifications can be made to the technical solutions of the present invention, including combinations of various technical features in any other suitable manner. These simple modifications and combinations should also be considered as the content disclosed in the present invention and are all within the protection scope of the present invention.

Claims

1. A method for preparing trichloromethanesulfonic acid, characterized in that, The raw materials are methanesulfonic acid and chlorine, with a molar ratio of 1:3-10. The methanesulfonic acid and chlorine are added to the reactor, and the raw materials in the reactor are irradiated and heated to a temperature of 150-500℃. In the tubular reactor, the methanesulfonic acid is chlorinated with chlorine to obtain trichloromethanesulfonic acid.

2. The method for preparing trichloromethanesulfonic acid according to claim 1, characterized in that, The reactor is a tubular reactor. The raw materials, methanesulfonic acid and chlorine, react inside the outer tube of the tubular reactor. The outer tube is exposed to light, while the inner tube is circulated with a temperature-controlled medium.

3. The method for preparing trichloromethanesulfonic acid according to claim 2, characterized in that, The inner diameter of the tubular reactor is 5-20 mm, the inner diameter of the outer tube is 2-5 mm larger than that of the inner tube, and the length-to-diameter ratio of the inner tube is 500-3000.

4. The method for preparing trichloromethanesulfonic acid according to claim 1, characterized in that, The illumination uses ultraviolet lamps with a power of 10-100W and a wavelength of 250-450nm.

5. The method for preparing trichloromethanesulfonic acid according to claim 2, characterized in that, The feed rate of methanesulfonic acid is 0.2-3 g / min.

6. The method for preparing trichloromethanesulfonic acid according to claim 2, characterized in that, The temperature control medium is heat transfer oil, which can be silicone oil, mineral oil, or synthetic oil.

7. The method for preparing trichloromethanesulfonic acid according to claim 1, characterized in that, The temperature for high-temperature heating is 150-500℃.

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